Sodium methanethiolate → 4-Chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

HRID 799

反応式

HRID 799 の反応式
[CH3:1][S-:2].[Na+].[Cl:4][C:5]1[CH:10]=[C:9](Cl)[N:8]=[C:7]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]=1>C1COCC1>[Cl:4][C:5]1[CH:10]=[C:9]([S:2][CH3:1])[N:8]=[C:7]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]=1

参加物

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 196938984,6-Dichloro-2-(phenylmethoxy)pyrimidine

生成物 1

HCID 196938764-Chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Aqueous sodium thiomethoxide (15%, 2.75 g, 0.0059×1.0 mol) was added dropwise in 4,6-dichloro-2-(phenylmethoxy)pyrimidine (Compound No. II-26) (1.5 g, 0.0059 mol) dissolved in THF at room temperature. After allowed to react for 2 hours, the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, then purified on a silica gel column to obtain 4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine (Compound No. II-15) as an intermediate.

後処理

  1. customto react for 2 hours
  2. customthe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
  3. washThe organic layer was washed with aqueous saturated sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. custompurified on a silica gel column

出典と根拠

ORDレコード
ord-bbaa547034cb4578bce2648d1c091a1f
出典データセット
uspto-grants-1998_03
特許番号
US05723412

関連ノート

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